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DOC316.53.01319
Method 10254
Reagent Solution
Adapted from Standard Methods for the Examination of Water and Wastewater.
Test preparation
Instrument-specific information
Table 1 shows all of the instruments that have the program for this test. The table also
shows sample cell and orientation requirements for reagent addition tests, such as
powder pillow or bulk reagent tests.
To use the table, select an instrument, then read across to find the applicable information
for this test.
Table 1 Instrument-specific information
Instrument
Sample cell
DR 6000
2495402
DR 3800
DR 2800
DR 2700
DR 1900
DR 5000
DR 3900
DR 900
2401906
Before starting
Samples must be analyzed immediately after collection and cannot be preserved for later analysis.
Install the instrument cap on the DR 900 cell holder before ZERO or READ is pushed.
Some sulfide loss can occur if dilution is necessary.
Review the Safety Data Sheets (MSDS/SDS) for the chemicals that are used. Use the recommended personal protective
equipment.
Dispose of reacted solutions according to local, state and federal regulations. Refer to the Safety Data Sheets for disposal
information for unused reagents. Refer to the environmental, health and safety staff for your facility and/or local regulatory
agencies for further disposal information.
Items to collect
Description
Quantity
Sulfide 1 Reagent
12 mL
Sulfide 2 Reagent
12 mL
Quantity
Sample cells (For information about sample cells, adapters or light shields, refer to Instrumentspecific information on page 1.)
Stoppers
Water, deionized
10 mL
Sample collection
Samples must be analyzed immediately after collection and cannot be preserved for
later analysis.
Collect samples in clean glass or plastic bottles with tight-fitting caps. Completely fill
the bottle and immediately tighten the cap.
Prevent agitation of the sample or exposure to air.
Start
4. Spectrophotometers:
Add deionized water to the
10-mL line. Colorimeters:
Add deionized water to the
25-mL line.
To prevent sulfide loss, do
not mix the sample more
than necessary.
6. Swirl to mix.
Zero
Read
Spectrophotometer volume
Colorimeter volume
10 mL
25 mL
1.0 mL
2.5 mL
0.1 mL
0.25 mL
is diluted by a factor of 10, the instrument multiplies the result by 10 and shows the
calculated result in the instrument display.
1. Select Options>More>Dilution factor from the instrument menu.
Note: DR 1900: Select Options>Advanced Options>Dilution Factors>On.
Note: Colorimeters include a dilution factor when the chemical form is set. Go to
Options>Advanced Options>Chemical Form and select LR, MR or HR.
Soluble sulfides
To measure soluble sulfides, use a centrifuge to separate the solids. To make an
estimate of the amount of insoluble sulfides in the sample, subtract the soluble sulfide
concentration from the total (with solids) sulfide concentration.
1. Fill a centrifuge tube completely with sample and immediately cap the tube.
2. Put the tube in a centrifuge and run the centrifuge to separate the solids.
3. Use the supernatant as the sample in the test procedure.
Interferences
Interfering
substance
Interference level
Barium
Concentrations more than 20 mg/L barium react with the sulfuric acid in Sulfide 1 Reagent and form a
BaSO4 (barite) precipitate. To correct for this interference:
1.
2.
3.
4.
5.
6.
7.
Spectrophotometers: use a 0.1-mL or 1.0-mL sample volume and add deionized water to the 10mL mark.
Colorimeters: use a 0.25-mL or 2.5-mL sample volume and add deionized water to the 25-mL
mark.
Add both Sulfide 1 and Sulfide 2 reagents per the procedure steps.
After the 5-minute reaction period, pour the sample into a 50-mL beaker.
Pull the sample into a Luer-Lock syringe (10 cc for spectrophotometers or 60 cc for colorimeters).
Put a 0.45-m filter disc on the Luer-Lock tip and filter the sample into a clean sample cell for
measurement. Use deionized water to prepare the blank.
Set the instrument zero and read the result, per the procedure steps.
Multiply by the appropriate dilution factor for the dilution used (10 or 100).
Strong reducing Prevent the full color development or reduce the blue color
substances such
as sulfite,
thiosulfate and
hydrosulfite
Sulfide, high
levels
High concentrations of sulfide can inhibit the full color development. Use a diluted sample in the test
procedure. Some sulfide loss can occur when the sample is diluted.
Turbidity
Pre-treat the sample to remove sulfide, then use the pre-treated sample as the blank in the test procedure.
Prepare a sulfide-free blank as follows:
1.
2.
3.
4.
Accuracy check
Standard solution method
Sulfide standard solutions are not stable and must be prepared by the user. Refer to
Standard Methods, 4500S2 for preparation and standardization instructions.
Method performance
The method performance data that follows was derived from laboratory tests that were
measured on a spectrophotometer during ideal test conditions. Users can get different
results under different test conditions.
Program
Standard
Sensitivity
Concentration change per 0.010 Abs change
691
0.52 mg/L S2
0.500.54 g/L S2
0.005 mg/L S2
Summary of method
Hydrogen sulfide and acid-soluble metal sulfides react with N,N-dimethyl-pphenylenediamine sulfate to form methylene blue. The intensity of the blue color is
proportional to the sulfide concentration. High sulfide levels in oil field waters may be
determined after proper dilution. The measurement wavelength is 665 nm for
spectrophotometers or 610 nm for colorimeters.
Quantity/test
Unit
Item no.
varies
4L
27256
2244500
Sulfide 1 Reagent
12 mL
100 mL MDB
181632
Sulfide 2 Reagent
12 mL
100 mL MDB
181732
Quantity/test
Unit
Item no.
each
1970001
50/pkg
2185696
each
1970010
varies
50/pkg
2199796
each
BBP078
100/pkg
BBP079
each
BBP065
75/pkg
BBP068
Water, deionized
Sulfide Reagent Set
Includes:
Required apparatus
Description
Unit
Item no.
Beaker, 50-mL
each
50041H
29 mL
221120
each
2088638
each
50541
29 mL
211220
each
53238
each
1465100
each
2202400
2258700
50/pkg
2513603
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01/2014, Edition 10